WO1987005110A1 - Lampe a decharge luminescente et son utilisation - Google Patents

Lampe a decharge luminescente et son utilisation Download PDF

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Publication number
WO1987005110A1
WO1987005110A1 PCT/DE1987/000063 DE8700063W WO8705110A1 WO 1987005110 A1 WO1987005110 A1 WO 1987005110A1 DE 8700063 W DE8700063 W DE 8700063W WO 8705110 A1 WO8705110 A1 WO 8705110A1
Authority
WO
WIPO (PCT)
Prior art keywords
chamber body
glow discharge
discharge lamp
anode
sample
Prior art date
Application number
PCT/DE1987/000063
Other languages
German (de)
English (en)
Inventor
Jae Bak; KO
Original Assignee
Gesellschaft Zur Förderung Der Spektrochemie Und A
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Gesellschaft Zur Förderung Der Spektrochemie Und A filed Critical Gesellschaft Zur Förderung Der Spektrochemie Und A
Priority to DE8787901348T priority Critical patent/DE3781065D1/de
Priority to KR1019870700982A priority patent/KR960016169B1/ko
Priority to AT87901348T priority patent/ATE79471T1/de
Publication of WO1987005110A1 publication Critical patent/WO1987005110A1/fr

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
    • G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J61/00—Gas-discharge or vapour-discharge lamps
    • H01J61/64—Cathode glow lamps

Definitions

  • the invention relates to a glow discharge lamp according to the preamble of patent claim 1 and its use according to patent claim 9.
  • Glow discharge lamps have found wide application in metal analysis by atomic emission spectroscopy (AES).
  • AES atomic emission spectroscopy
  • an electrically conductive sample to be examined is connected to an anode, a gas capable of glow discharge, preferably an inert gas under low pressure, being located in the space between the cathode and the anode.
  • the occurrence of the glow discharge depends on the ratio of both the operating voltage, the current and the gas pressure between the cathode and the anode.
  • the radiation from the glow discharge is observed through a window which is usually arranged above the anode, and information about the content of certain elements in the sample is obtained from its spectral analysis.
  • a glow discharge lamp is known from German patent application P 34 29 765, in which a carrier gas flows through an inner gas space and a glow discharge occurs in the gas space when a voltage is applied between the anode and cathode.
  • the sample is connected as part of the cathode, while a transparent housing part is used for the spectral analysis of the glow discharge light.
  • the anode is partially embedded in a solid, non-conductive body and is at high voltage potential, while the sample - as cathode - is at zero potential.
  • the short-circuit strength of the housing of the glow lamp can be ensured in the simplest way.
  • this prior art mög ⁇ Lich to place the anode at a high voltage and the cathode at zero potential, whereby a light and risk-free "Replacing the sample is made possible.
  • the non-conductive material in the gas space is achieved that quickly adjust the walls of the discharge space to the temperature in the gas space, since electrically non-conductive material is generally also poorly heat-conductive, and this known arrangement ensures rapid setting of constant measurement conditions and reproducible results.
  • the invention is therefore based on the object of developing the known glow discharge lamps while lowering the detection limit in atomic emission spectroscopy in such a way that the use of other spectroscopic methods by means of which excited atoms, such as those present in a glow discharge, can be examined, is also investigated enable.
  • a solution to this problem according to the invention is characterized by its developments in the claims.
  • the invention is based on the idea of observing the glow discharge also through a side window. Because, in contrast to previously known glow discharge lamps, side windows are now provided for the first time, which also allow lateral observation of the glow light, possibly after optical excitation by incident radiation, the glow discharge lamp can now also be used for other spectroscopic methods, such as the atom -Fluorescence spectroscopy or the like. It is also possible to attach a light guide or the like to the side window. to be connected in order to investigate the emerging radiation, if necessary spatially further away.
  • the chamber body has a first gas supply line emerging in the area of the negative glow light, a first vacuum line arranged above the first gas supply line, a second, optionally closable, arranged between the first gas supply line and below the anode embedded in the chamber body re gas supply line and a third, arranged between the anode and the end of the gas supply line.
  • a further line is provided on the end part, to which both vacuum and the gas supply can be connected. Due to the geometrically balanced reinforcement of the bushings for vacuum and the gas feeds, a uniform pressure distribution above the sample and thus a plane-parallel sample removal can be achieved, as is particularly desired for surface and depth profile analyzes.
  • the different arrangement of the lines also makes it possible to adapt the design of the sample crater to the analysis requirements - surface analysis, depth analysis or to certain material conditions - rough, uneven surface with high release energies or low release energies.
  • an interchangeable insert part can be arranged in the cathode part holding the sample, which through its inner opening surrounds the sample section exposed to the vacuum or the removal of materials.
  • This section can be controlled in any way by the choice of the insert, depending on whether small sections of the sample are to be examined or whether the removal is as flat as possible.
  • the reservoir of free atoms can be used for methods of atomic absorption spectroscopy, atomic fluorescence spectral copy and LEI ("laser-enhanced ionization").
  • LEI laser-enhanced ionization
  • FIG. 1 shows the essential parts of a glow discharge lamp according to the invention, cut along the anode / cathode connecting line;
  • FIG. 2 shows the sample-side part of the glow discharge lamp of FIG. 1, cut along the vacuum line;
  • FIG. 3 shows two enlarged sections of possible preferred embodiments of the sample area of a glow discharge lamp according to the invention.
  • FIG. 4 shows a further preferred embodiment of the glow discharge lamp according to the invention in the region of the end part, with a shielded anode.
  • the glow discharge lamp according to the invention has a sample 2 which is fastened to a cathode part 3 in a sealing manner by means of a seal, for example an O-ring seal.
  • the cathode part adjoins the chamber body 4 made of non-conductive material, preferably a ceramic material, in which a first gas supply line 5, which ends just above the sample, a first vacuum line 6, which is above the first gas supply line is arranged, a second gas supply line 7, preferably with a lower transverse Cut as the first gas supply line, an anode 8 embedded in the chamber body 4 and a third gas supply line 11 are provided, which supply argon above the anode, below the end part 12. All lines open into a gas interior.
  • a through opening, the gas interior GR, is formed in the chamber body 4, which, in this preferred embodiment, increases in the shape of a truncated cone in the direction of the anode, starting from the sample 2.
  • the anode has an internal opening that is aligned with the axis of the gas interior.
  • the gas interior (GR) is closed off by a closing part 12, which can be a window, for example, and which can optionally have a further line for gas supply or vacuum connection, and in the embodiment shown here is also connected via O- Sealed rings.
  • At least one lateral observation window 18 is formed in the cathode part, through which the negative glow light developing above the sample can be observed in the gas interior.
  • a further observation window can be provided, which can also be used to introduce rays, for example excitation radiation in the UV (ultraviolet) or VIS (visible) range.
  • the introduction of radiation to excite the atoms present in the negative glow light can also take place through the end window 12 and can be observed from the side.
  • the observation window 18 is replaced by an optical waveguide which enables connection to a spectrometer which is relatively far away.
  • an aligned arrangement can also an irradiation opening and an observation opening can be provided.
  • the surface area of the sample exposed to the detection method is preferably limited by an insert 15, as shown in FIG. 2. It is possible to change the inside opening of the sample part according to the method used or the type of analysis result desired.
  • FIG. 3 shows the sample area of two embodiments of the glow lamp according to the invention in a representative manner enlarged (different on the left and right), the insert part 15 being provided with an opening 17 for an operating mode in which a further part part 16 is provided is designed to be interchangeable.
  • An opening 17 is provided in the divider part 16, through which a part or the total amount of the carrier gas, depending on the intended use, can flow into the chamber.
  • the distance between the 'end face of the insert part 15 in front of the sample for example, 0.01 mm to 0.5, preferably less than 0.2 mm.
  • the anode 8 is shielded from the gas interior by a partition wall 21.
  • the shielded anode procedure is advantageous in some preferred applications of the glow discharge lamp according to the invention. It is preferred if no metallic or conductive parts on the anode 8 and the sample 2 limit the gas interior.
  • the glow discharge lamp according to the invention is operated by charging the openings 5 and 11 with argon and applying a vacuum to the opening 6 at high voltage (sample as cathode at zero potential, anode at high voltage potential).
  • the noble gas supply conduits 5, 7 and 17 are closed and noble gas only enters through the opening 11 while a vacuum is being drawn through the opening 6.
  • the latter mode of operation is particularly suitable for samples made of aluminum-silicon alloys which are very poorly degradable and poorly conductive, as occurs generally in the case of high-melting substances with high binding energy.
  • the noble gas supply 11 As well as the line 17 and to supply noble gas only via the lines 5 and 7, while a vacuum is drawn through the opening 6.
  • the inventive design of the glow discharge lamp makes it possible for the first time to measure not only end-on but also side-on, the negative glow light being formed at a distance of 0.5 to 20 mm above the sample.
  • the openings 5 in the chamber body are provided approximately in the plasma plane.
  • Known light sources can be used as primary radiation sources in connection with the glow discharge lamp according to the invention in atomic absorption sorption spectroscopy or atomic fluorescence spectroscopy.
  • light sources can be used which emit light with a narrow line width and high coherence.
  • the line width of the light emitted by the light source is typically an order of magnitude smaller than the width of the absorption line: for example, the line width of the light from the light source can be between 5 and 500 MHz, preferably between 10 and 50 MHz.
  • tunable temperature-stabilized semiconductor lasers are preferably used as light sources.
  • the glow discharge lamp according to the invention makes it possible for the first time to increase the analytical performance to an unprecedented extent by changing the height of the radiation guidance above the sample and thus the relevant discharge layer.
  • the arrangement according to the invention makes it possible to use the gas discharges at reduced pressure not only for the optical emission spectroscopic method (OES), but rather also for other proven methods, such as atomic absorption (AAS), atomic fluorescence spectroscopy (AFS) and the optogalvanic method (LEI) analytically.
  • the glow discharge lamp according to the invention lowers the limits of the trace analysis at the OES.
  • the arrangement according to the invention makes it possible for the first time to use glow discharge lamps in methods other than OES.

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  • Health & Medical Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

Une lampe à décharge luminescente est munie d'un corps de chambre possédant une ou plusieurs ouvertures d'admission et d'aspiration sous vide du gaz, ledit corps de chambre étant réalisé dans un matériau isolant et comportant un espace pour le gaz s'étendant en direction de l'anode et limité latéralement par la paroi interne du corps de chambre. La lampe comprend également une éprouvette disposée au niveau de l'extrémité cathodique du corps de chambre, ainsi qu'une anode logée dans le corps de chambre. L'éprouvette est de préférence maintenue au potentiel zéro et ladite anode comportant une ouverture de passage est de préférence maintenue sous haute tension. L'anode est également pourvue d'un élément de fermeture situé à l'extrémité du corps de chambre et conçu éventuellement comme une fenêtre d'observation, au moins une ouverture de regard (18) étant disposée latéralement dans le corps de chambre (4), à environ la hauteur de la lueur de décharge négative, une fermeture hermétique de l'espace intérieur destinée au gaz au niveau de l'extrémité cathodique étant assurée par l'éprouvette (2).
PCT/DE1987/000063 1986-02-24 1987-02-24 Lampe a decharge luminescente et son utilisation WO1987005110A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DE8787901348T DE3781065D1 (de) 1986-02-24 1987-02-24 Glimmentladungslampe sowie deren verwendung.
KR1019870700982A KR960016169B1 (ko) 1986-02-24 1987-02-24 글로우 방전램프
AT87901348T ATE79471T1 (de) 1986-02-24 1987-02-24 Glimmentladungslampe sowie deren verwendung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DEP3605911.0 1986-02-24
DE19863605911 DE3605911A1 (de) 1986-02-24 1986-02-24 Glimmentladungslampe sowie ihre verwendung

Publications (1)

Publication Number Publication Date
WO1987005110A1 true WO1987005110A1 (fr) 1987-08-27

Family

ID=6294824

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/DE1987/000063 WO1987005110A1 (fr) 1986-02-24 1987-02-24 Lampe a decharge luminescente et son utilisation

Country Status (7)

Country Link
US (1) US4830492A (fr)
EP (1) EP0258331B1 (fr)
JP (1) JP2530189B2 (fr)
KR (1) KR960016169B1 (fr)
AU (1) AU7081487A (fr)
DE (2) DE3605911A1 (fr)
WO (1) WO1987005110A1 (fr)

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US5405514A (en) * 1993-07-28 1995-04-11 Gas Research Institute Atmospheric pressure gas glow discharge
US20030047146A1 (en) * 2001-09-10 2003-03-13 Daniel Michael J. Plasmatron-internal combustion engine system having an independent electrical power source
US6959542B2 (en) * 2002-01-25 2005-11-01 Arvin Technologies, Inc. Apparatus and method for operating a fuel reformer to regenerate a DPNR device
US7014930B2 (en) * 2002-01-25 2006-03-21 Arvin Technologies, Inc. Apparatus and method for operating a fuel reformer to generate multiple reformate gases
US7021048B2 (en) * 2002-01-25 2006-04-04 Arvin Technologies, Inc. Combination emission abatement assembly and method of operating the same
US6976353B2 (en) * 2002-01-25 2005-12-20 Arvin Technologies, Inc. Apparatus and method for operating a fuel reformer to provide reformate gas to both a fuel cell and an emission abatement device
US6651597B2 (en) * 2002-04-23 2003-11-25 Arvin Technologies, Inc. Plasmatron having an air jacket and method for operating the same
WO2003091551A1 (fr) * 2002-04-24 2003-11-06 Arvin Technologies, Inc. Dispositif et procede de regeneration d'un filtre a particules d'un systeme d'echappement d'un moteur a combustion interne
US6881386B2 (en) * 2002-05-30 2005-04-19 Massachusetts Institute Of Technology Low current plasmatron fuel converter having enlarged volume discharges
US20040020188A1 (en) * 2002-08-05 2004-02-05 Kramer Dennis A. Method and apparatus for generating pressurized air by use of reformate gas from a fuel reformer
US20040020191A1 (en) * 2002-08-05 2004-02-05 Kramer Dennis A. Method and apparatus for advancing air into a fuel reformer by use of a turbocharger
US20040020447A1 (en) * 2002-08-05 2004-02-05 William Taylor Method and apparatus for advancing air into a fuel reformer by use of an engine vacuum
WO2004015511A1 (fr) * 2002-08-12 2004-02-19 Arvin Technologies, Inc. Appareil et procede d'ajustement du rapport oxygene-carbone d'un reformeur de combustible
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US6758035B2 (en) * 2002-09-18 2004-07-06 Arvin Technologies, Inc. Method and apparatus for purging SOX from a NOX trap
US20040052693A1 (en) * 2002-09-18 2004-03-18 Crane Samuel N. Apparatus and method for removing NOx from the exhaust gas of an internal combustion engine
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US6715452B1 (en) 2002-11-13 2004-04-06 Arvin Technologies, Inc. Method and apparatus for shutting down a fuel reformer
US6903259B2 (en) * 2002-12-06 2005-06-07 Arvin Technologies, Inc. Thermoelectric device for use with fuel reformer and associated method
US20040139730A1 (en) * 2003-01-16 2004-07-22 William Taylor Method and apparatus for directing exhaust gas and reductant fluid in an emission abatement system
US6843054B2 (en) * 2003-01-16 2005-01-18 Arvin Technologies, Inc. Method and apparatus for removing NOx and soot from engine exhaust gas
US20040144030A1 (en) * 2003-01-23 2004-07-29 Smaling Rudolf M. Torch ignited partial oxidation fuel reformer and method of operating the same
US6851398B2 (en) * 2003-02-13 2005-02-08 Arvin Technologies, Inc. Method and apparatus for controlling a fuel reformer by use of existing vehicle control signals
US7407634B2 (en) * 2003-04-11 2008-08-05 Massachusetts Institute Of Technology Plasmatron fuel converter having decoupled air flow control
US20040216378A1 (en) * 2003-04-29 2004-11-04 Smaling Rudolf M Plasma fuel reformer having a shaped catalytic substrate positioned in the reaction chamber thereof and method for operating the same
US7244281B2 (en) * 2003-10-24 2007-07-17 Arvin Technologies, Inc. Method and apparatus for trapping and purging soot from a fuel reformer
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US7381382B2 (en) * 2004-03-29 2008-06-03 Massachusetts Institute Of Technology Wide dynamic range multistage plasmatron reformer system
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Also Published As

Publication number Publication date
EP0258331A1 (fr) 1988-03-09
US4830492A (en) 1989-05-16
AU7081487A (en) 1987-09-09
EP0258331B1 (fr) 1992-08-12
KR880700930A (ko) 1988-04-13
KR960016169B1 (ko) 1996-12-04
DE3605911A1 (de) 1987-08-27
JP2530189B2 (ja) 1996-09-04
JPS63503009A (ja) 1988-11-02
DE3781065D1 (de) 1992-09-17

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